#------------------------------------------------------------------------------
#$Date: 2016-12-18 19:17:40 +0200 (Sun, 18 Dec 2016) $
#$Revision: 189196 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/18/4331891.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4331891
loop_
_publ_author_name
'Hudson, Timothy A.'
'Berry, Kevin J.'
'Moubaraki, Boujemaa'
'Murray, Keith S.'
'Robson, Richard'
_publ_section_title
;
 Citrate, in Collaboration with a Guanidinium Ion, as a Generator of
 Cubane-like Complexes with a Range of Metal Cations: Synthesis,
 Structures, and Magnetic Properties of
 [C(NH2)3]8[(MII)4(cit)4]·8H2O (M = Mg, Mn, Fe, Co, Ni, and Zn; cit
 = Citrate)
;
_journal_issue                   9
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3549
_journal_page_last               3556
_journal_paper_doi               10.1021/ic051779m
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety
;
1(Mn 2+), 1(C6 H4 O7 4-), 2(C H6 N3 1+), 2(H2 O)
;
_chemical_formula_sum            'C8 H20 Mn N6 O9'
_chemical_formula_weight         399.24
_chemical_name_systematic        ?
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.2890(12)
_cell_length_b                   16.2890(12)
_cell_length_c                   11.5022(17)
_cell_measurement_reflns_used    2433
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.2
_cell_volume                     3051.9(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18319
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, G. M.  SADABS'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0862
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0848P)²+14.9271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1973
_refine_ls_wR_factor_ref         0.2135
_reflns_number_gt                2645
_reflns_number_total             3480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051779msup1.cif
_cod_data_source_block           mncitrate
_cod_original_sg_symbol_H-M      P42/n
_cod_database_code               4331891
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_attached_hydrogens
C1 C 0.0971(4) 0.3107(4) 0.8999(5) 0.0387(14) Uani 1 1 d . 0
C3 C 0.1040(4) 0.4038(4) 0.9306(5) 0.0384(13) Uani 1 1 d . 0
H7 H 0.1215 0.4344 0.8626 0.06(2) Uiso 1 1 calc R 0
H8 H 0.0508 0.4246 0.9547 0.07(2) Uiso 1 1 calc R 0
C4 C 0.1668(4) 0.4154(4) 1.0297(5) 0.0455(16) Uani 1 1 d . 0
O6 O 0.4143(2) 0.3654(2) 0.9025(4) 0.0345(9) Uani 1 1 d . 0
C2 C 0.0175(4) 0.3070(3) 0.8191(5) 0.0349(13) Uani 1 1 d . 0
C7 C 0.6562(3) 0.3262(3) 0.6452(5) 0.0309(12) Uani 1 1 d . 0
C8 C 0.0075(3) 0.4104(3) 0.3574(5) 0.0320(12) Uani 1 1 d . 0
C6 C 0.0481(4) 0.1782(3) 0.9820(6) 0.0389(14) Uani 1 1 d . 0
O1 O 0.1698(2) 0.2839(2) 0.8403(3) 0.0267(8) Uani 1 1 d . 0
O5 O 0.1428(3) 0.4405(3) 1.1252(4) 0.0509(13) Uani 1 1 d . 0
O4 O 0.2424(2) 0.3968(2) 1.0086(3) 0.0326(9) Uani 1 1 d . 0
O2 O 0.0296(2) 0.2933(2) 0.7141(3) 0.0288(8) Uani 1 1 d . 0
O3 O -0.0515(3) 0.3126(3) 0.8644(4) 0.0476(11) Uani 1 1 d . 0
C5 C 0.0844(4) 0.2614(3) 1.0108(6) 0.0393(14) Uani 1 1 d . 0
H9 H 0.1366 0.2542 1.0502 0.020(13) Uiso 1 1 calc R 0
H10 H 0.0478 0.2908 1.0626 0.08(3) Uiso 1 1 calc R 0
O7 O -0.0134(3) 0.1551(3) 1.0372(5) 0.0570(14) Uani 1 1 d . 0
Mn1 Mn 0.29004(5) 0.34477(5) 0.84952(7) 0.0262(3) Uani 1 1 d . 0
N1 N 0.5970(3) 0.2911(3) 0.5853(4) 0.0367(11) Uani 1 1 d . 0
H1A H 0.5620 0.2600 0.6198 0.039(18) Uiso 1 1 calc R 0
H1B H 0.5934 0.2992 0.5116 0.09(3) Uiso 1 1 calc R 0
N2 N 0.6614(3) 0.3134(3) 0.7585(4) 0.0352(11) Uani 1 1 d . 0
H2A H 0.6262 0.2823 0.7926 0.05(2) Uiso 1 1 calc R 0
H2B H 0.7000 0.3362 0.7980 0.05(2) Uiso 1 1 calc R 0
N3 N 0.7116(3) 0.3732(3) 0.5936(5) 0.0414(12) Uani 1 1 d . 0
H3A H 0.7092 0.3813 0.5198 0.06(2) Uiso 1 1 calc R 0
H3B H 0.7499 0.3958 0.6339 0.07(3) Uiso 1 1 calc R 0
N4 N -0.0158(3) 0.4748(3) 0.2955(5) 0.0385(12) Uani 1 1 d . 0
H4A H -0.0551 0.5056 0.3200 0.06(2) Uiso 1 1 calc R 0
H4B H 0.0083 0.4859 0.2309 0.038(18) Uiso 1 1 calc R 0
N5 N -0.0286(3) 0.3929(3) 0.4557(4) 0.0380(12) Uani 1 1 d . 0
H5A H -0.0680 0.4234 0.4807 0.029(16) Uiso 1 1 calc R 0
H5B H -0.0131 0.3510 0.4953 0.05(2) Uiso 1 1 calc R 0
N6 N 0.0672(3) 0.3627(3) 0.3179(4) 0.0398(12) Uani 1 1 d . 0
H6A H 0.0821 0.3203 0.3569 0.06(2) Uiso 1 1 calc R 0
H6B H 0.0910 0.3743 0.2531 0.07(3) Uiso 1 1 calc R 0
O8 O 0.1927(3) 0.5950(3) 1.1792(4) 0.0497(12) Uani 1 1 d . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 C1 C5 110.6(5) . .
O1 C1 C3 110.0(4) . .
C5 C1 C3 109.4(5) . .
O1 C1 C2 112.4(4) . .
C5 C1 C2 111.0(5) . .
C3 C1 C2 103.2(5) . .
C4 C3 C1 109.5(5) . .
O5 C4 O4 123.1(6) . .
O5 C4 C3 119.2(6) . .
O4 C4 C3 117.7(5) . .
C6 O6 Mn1 123.8(3) 2 .
O3 C2 O2 124.4(6) . .
O3 C2 C1 119.2(5) . .
O2 C2 C1 116.2(5) . .
N1 C7 N2 119.6(5) . .
N1 C7 N3 121.0(6) . .
N2 C7 N3 119.3(5) . .
N5 C8 N4 120.6(5) . .
N5 C8 N6 120.0(5) . .
N4 C8 N6 119.4(5) . .
O7 C6 O6 124.7(5) . 2
O7 C6 C5 118.2(6) . .
O6 C6 C5 117.1(5) 2 .
C1 O1 Mn1 125.1(3) . .
C1 O1 Mn1 111.8(3) . 8_657
Mn1 O1 Mn1 97.14(13) . 8_657
C1 O1 Mn1 120.7(3) . 2
Mn1 O1 Mn1 99.36(14) . 2
Mn1 O1 Mn1 97.09(13) 8_657 2
C4 O4 Mn1 126.4(4) . .
C2 O2 Mn1 118.8(4) . 8_657
C6 C5 C1 109.9(5) . .
O6 Mn1 O4 92.11(15) . .
O6 Mn1 O2 85.73(14) . 7_567
O4 Mn1 O2 85.68(14) . 7_567
O6 Mn1 O1 158.02(14) . .
O4 Mn1 O1 84.14(13) . .
O2 Mn1 O1 115.45(14) 7_567 .
O6 Mn1 O1 110.03(15) . 7_567
O4 Mn1 O1 150.14(14) . 7_567
O2 Mn1 O1 76.62(13) 7_567 7_567
O1 Mn1 O1 82.11(14) . 7_567
O6 Mn1 O1 83.23(13) . 2
O4 Mn1 O1 121.45(14) . 2
O2 Mn1 O1 150.94(14) 7_567 2
O1 Mn1 O1 80.36(14) . 2
O1 Mn1 O1 82.07(14) 7_567 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.437(7) .
C1 C5 1.522(9) .
C1 C3 1.561(8) .
C1 C2 1.596(8) .
C3 C4 1.544(9) .
C4 O5 1.236(7) .
C4 O4 1.291(8) .
O6 C6 1.309(7) 2
O6 Mn1 2.140(4) .
C2 O3 1.241(7) .
C2 O2 1.244(7) .
C7 N1 1.317(7) .
C7 N2 1.322(7) .
C7 N3 1.324(7) .
C8 N5 1.306(7) .
C8 N4 1.324(7) .
C8 N6 1.324(8) .
C6 O7 1.245(7) .
C6 O6 1.309(7) 2
C6 C5 1.515(8) .
O1 Mn1 2.197(3) .
O1 Mn1 2.198(4) 8_657
O1 Mn1 2.199(4) 2
O4 Mn1 2.160(4) .
O2 Mn1 2.173(4) 8_657
Mn1 O2 2.173(4) 7_567
Mn1 O1 2.198(4) 7_567
Mn1 O1 2.199(4) 2
